CN113881864A - Rapid preparation method of high-thermal-conductivity tungsten copper - Google Patents
Rapid preparation method of high-thermal-conductivity tungsten copper Download PDFInfo
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- CN113881864A CN113881864A CN202110657386.3A CN202110657386A CN113881864A CN 113881864 A CN113881864 A CN 113881864A CN 202110657386 A CN202110657386 A CN 202110657386A CN 113881864 A CN113881864 A CN 113881864A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
Abstract
The invention discloses a rapid preparation method of high-thermal conductivity tungsten copper, which prepares tungsten copper with high density and strong electric and thermal conductivity in a short time. The method comprises the following steps: filling pure tungsten powder and copper powder filler into the surface of the powder after filling; regulating the gas pressure to be between 0.3 and 0.6Kg under vacuum or inert gas, and mixing materials; after the mixing is finished, carrying out deoxidation treatment on the powder; filling powder into a mould, and sintering: a pre-pressing section: maintaining the pressure for 10-60s under the condition of pre-pressing of 20 MPa; a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃; after the plasticizing state is finished, heating to 860 ℃ and 1020 ℃ at the heating rate of 20-22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder; a pressure maintaining section: sintering at 1063-1080 ℃ and under a pressureless state; and cooling for 2 hours to finish the preparation of the tungsten copper.
Description
Technical Field
The invention relates to the technical field of workpiece forming, in particular to a rapid preparation method of high-thermal-conductivity tungsten copper.
Background
The tungsten-copper alloy is an alloy of tungsten and copper, the tungsten and the copper are mutually insoluble, the tungsten-copper alloy is a pseudo alloy which is extremely difficult to form and compact, belongs to a metal-based composite material, and can be applied to the important fields of aerospace, aviation, electronics and the like.
The tungsten element and the copper element are not mutually soluble, so the performance of the tungsten element can be effectively embodied, and the tungsten element comprises low expansibility, wear resistance, corrosion resistance, high electric and thermal conductivity, high strength and certain plasticity.
The infiltration method is widely adopted in the market, and tungsten copper produced by the infiltration method has higher density and good sintering performance, and has the defects that redundant infiltrated metal copper needs to be removed by machining after infiltration, the processing cost is increased, the yield is not high, the powder is not uniformly dispersed and distributed, the compactness is loose, and the thermal conductivity is poor; a high-temperature sintering tungsten skeleton copper infiltration method is also adopted, and the method has high comprehensive performance, complex and complicated process, high production cost and no popularization; and the isostatic pressing process is adopted, so that the produced tungsten copper has good quality, but the cost is extremely high, and the method cannot be popularized.
Disclosure of Invention
The invention provides a rapid preparation method of high-thermal conductivity tungsten copper, which can prepare the tungsten copper with high density, high electric conductivity and high thermal conductivity in a short time.
The invention provides a rapid preparation method of high-thermal-conductivity tungsten copper, which comprises the following steps:
(1) filling pure tungsten powder and copper powder filler into the surface of the powder after filling;
(2) regulating the gas pressure to be between 0.3 and 0.6Kg under vacuum or inert gas, and mixing materials;
(3) after the mixing is finished, carrying out deoxidation treatment on the powder;
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 10-60s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 860 ℃ and 1020 ℃ at the heating rate of 20-22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063-1080 ℃ and under a pressureless state;
(5) cooling for 2 hours to finish the preparation of tungsten copper;
the preparation time of the steps (1) to (4) is 1.5 to 2.5 hours.
Preferably, the step (1) is specifically: taking pure tungsten powder and copper powder, placing the copper powder at the bottom, covering the copper powder (completely) with the pure tungsten powder to finish filling, and filling a mixing ball on the surface of the powder;
the mixing ball is an alloy ball or a ceramic ball.
Preferably, when the mixing balls are alloy balls, the weight ratio of the alloy balls to the powder is 3:1, and the ball diameter of the alloy balls is phi 10 or phi 18;
preferably, when the mixing ball is a ceramic ball, the weight ratio of the ceramic ball to the powder is 5:1, and the ball diameter of the ceramic ball is phi 3, phi 5 or phi 10; the ceramic balls are zirconium balls.
Preferably, the formula proportion of the tungsten copper is any one of Wcu10, Wcu20, Wcu30, Wcu40 and Wcu 50.
Preferably, the step (2) is specifically: when a vacuum method is adopted, the vacuum environment is 10-2And (3) mixing materials for 12 hours by adjusting the air pressure to be between 0.3 and 0.6 Kg.
Preferably, the step (2) is specifically: when an inert gas method is adopted, vacuumizing is firstly carried out for 3min, a vacuum valve is closed, an inflation valve is opened, inert gas is inflated, when the pressure is 1K +/-0.1, the inflation valve is closed, inflation is stopped, the air pressure is adjusted to be 0.3-0.6Kg, and the materials are mixed for 12-18 hours.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is simple and short in time, the time (single-furnace production time) can be shortened to 1.5-2.5 hours by different material mixing modes and sintering modes in the prior art, the time is short, the efficiency is high, the material distribution is uniform, the performance is stable, and the prepared tungsten copper has high density, high sintering performance, strong electrical conductivity and strong thermal conductivity.
Detailed Description
The following examples further describe embodiments of the present invention in detail. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The tungsten-copper alloy named in the application integrates tungstenThe melting point of tungsten element is as high as 3410 ℃, and the melting point of copper element is 1083 ℃; the density of tungsten element is as high as 19.35g/cm3The density of the copper element reaches 8.9g/cm3。
The tungsten-copper alloy is widely applied to military high-temperature-resistant materials, electric alloys for high-voltage switches, electric processing electrodes and microelectronic materials, and is widely applied to industries such as aerospace, aviation, electronics, electric power, metallurgy, machinery, sports equipment and the like as parts and components.
The invention discloses a rapid preparation method of high-thermal-conductivity tungsten copper, which comprises the following steps:
(1) filling pure tungsten powder and copper powder filler into the surface of the powder after filling;
(2) regulating the gas pressure to be between 0.3 and 0.6Kg under vacuum or inert gas, and mixing materials;
(3) after the mixing is finished, carrying out deoxidation treatment on the powder;
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 10-60s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 860 ℃ and 1020 ℃ at the heating rate of 20-22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063-1080 ℃ and under a pressureless state;
(5) cooling for 2 hours to finish the preparation of tungsten copper;
the preparation time of the steps (1) to (4) is 1.5 to 2.5 hours.
The steps can be carried out in a tank.
Preferably, the step (1) is specifically: taking pure tungsten powder and copper powder, placing the copper powder at the bottom, covering the copper powder (completely) with the pure tungsten powder to finish filling, and filling a mixing ball on the surface of the powder;
the mixing ball is an alloy ball or a ceramic ball.
Preferably, when the mixing balls are alloy balls, the weight ratio of the alloy balls to the powder is 3:1, and the ball diameter of the alloy balls is phi 10 or phi 18;
preferably, when the mixing ball is a ceramic ball, the weight ratio of the ceramic ball to the powder is 5:1, and the ball diameter of the ceramic ball is phi 3, phi 5 or phi 10; the ceramic balls are zirconium balls.
Preferably, the formula proportion of the tungsten copper is any one of Wcu10, Wcu20, Wcu30, Wcu40 and Wcu50 (unit is:%).
Preferably, the step (2) is specifically: when a vacuum method is adopted, the vacuum environment is 10-2And (3) mixing materials for 12 hours by adjusting the air pressure to be between 0.3 and 0.6 Kg.
Preferably, the step (2) is specifically: when an inert gas method is adopted, vacuumizing is firstly carried out for 3min, a vacuum valve is closed, an inflation valve is opened, inert gas is inflated, when the pressure is 1K +/-0.1, the inflation valve is closed, inflation is stopped, the air pressure is adjusted to be 0.3-0.6Kg, and the materials are mixed for 12-18 hours.
The preparation method can be used on an alternating-current high-power vacuum hot-pressing sintering furnace.
The preparation method of the invention is different from the preparation method of the background technology, and the powder is mixed according to the proportion. Pure tungsten powder and copper powder are in a weightless state in a processor (tank) under a vacuum state, and can be well and uniformly mixed under the coordination of mixing balls, so that the homogeneity of the powder is effectively ensured to reach the optimal mixing time, and the time is short. The mixing is carried out in an inert gas state, and the time required for the inert gas state is relatively long compared with the mixing in a vacuum state while maintaining the positive pressure.
Under the condition of vacuum or inert gas, the mixing efficiency of pure tungsten powder and copper powder is effectively enhanced under the action of the mixing balls.
Then the powder is filled into a die, and the uniformity of the powder filling is emphatically ensured.
And (4) charging and sintering, wherein the balance and consistency of the upper and lower pressure heads are kept during charging.
In the process of the temperature rise section, the powder is firstly quickly plasticized, and then the speed is slowly reduced, so that the forming effect can be effectively improved, and the effect of complete compactness is realized.
After the product is taken out of the furnace (step (6)), the product is subjected to high-temperature treatment, and is closer to a liquid phase and a sweating state, so that the stability of ductility performance is improved.
The pure tungsten powder and the copper powder are at low temperature in a vacuum state of the preparation method, so that the heating modes are different, the time for sintering the pure tungsten powder and the copper powder into the solution synthesis alloy is short, the high-efficiency continuity of the whole production prompts the preparation method to be different from the prior art, and the special process of the preparation method for sintering the powder ensures that the performance of the product is more consistent with a theoretical value, the material quality is more uniform, and the quality is more excellent.
The whole preparation method is short in time, simple and suitable for popularization and application.
Applicable fields include: tungsten-copper electrode, spot-discharging material, welding material,Guide and guardMaterials, electronic packaging, and the like. The method specifically comprises the following steps: the device comprises a tungsten-copper electronic packaging piece, a tungsten-copper heat conduction nozzle, a tungsten-copper electric contact, a tungsten-copper belt handle electrode, a tungsten-copper nut motor cover, a tungsten-copper electric welding electrode, an NDB tungsten-copper electrode, a tungsten-copper plasma electrode, a tungsten-copper electrode wheel and a tungsten-copper sealing cap electrode.
The rapid preparation method of the high-thermal-conductivity tungsten copper comprises the following steps:
(1) taking pure tungsten powder and copper powder as fillers, wherein the formula proportion of tungsten and copper is any one of Wcu10, Wcu20, Wcu30, Wcu40 and Wcu50, and filling a mixing ball on the surface of the filled powder;
the filling mode is that copper powder with low density is filled at the bottom, and pure tungsten powder with high density is filled to cover the copper powder, and the copper powder is completely covered to finish the filling.
Then, placing a mixing ball above the powder; the mixing ball is an alloy ball or a ceramic ball.
When the mixing ball is an alloy ball, the weight ratio of the alloy ball to the powder is 3:1, and the ball diameter of the alloy ball is phi 10 or phi 18;
when the mixing ball is a ceramic ball, the weight ratio of the ceramic ball to the powder is 5:1, and the ball diameter of the ceramic ball is phi 3, phi 5 or phi 10; the ceramic balls are zirconium balls;
(2) regulating the gas pressure to be between 0.3 and 0.6Kg under vacuum or inert gas, and mixing materials;
when a vacuum method is adopted, the vacuum environment is 10-2Regulating the air pressure to be 0.3-0.6Kg, mixing for 12 hours, and performing deoxidation treatment on the powder after the mixing is finished;
when an inert gas method is adopted, vacuumizing for 3min, closing a vacuum valve, opening an inflation valve, inflating inert gas, closing the inflation valve when the pressure is 1K +/-0.1, stopping inflating, adjusting the air pressure to be 0.3-0.6Kg, mixing materials, and carrying out deoxidation treatment on the powder after the mixing is finished for 12-18 hours (3);
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 10-60s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 860 ℃ and 1020 ℃ at the heating rate of 22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063-1080 ℃ and under a pressureless state;
(5) cooling for 2 hours to finish the preparation of tungsten copper;
the preparation time of the steps (1) to (4) is 1.5 to 2.5 hours.
The invention is illustrated by the following specific examples:
example 1
Preparing tungsten copper:
(1) taking pure tungsten powder and copper powder as fillers, wherein the formula of tungsten and copper is Wcu50, and filling the surface of the filled powder with a mixing ball;
the filling mode is as follows: filling copper powder at the bottom, filling pure tungsten powder to cover the copper powder, and completing filling;
then, placing a mixing ball above the powder; the mixing ball is an alloy ball.
The weight ratio of the alloy ball to the powder is 3:1, and the diameter of the alloy ball is phi 10;
(2) vacuum method, vacuum environment is 10-2Adjusting the air pressure to be 0.5Kg, mixing the materials for 12 hours, and performing deoxidation treatment on the powder after the materials are mixed;
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 50s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 1020 ℃ at a heating rate of 22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063 deg.c and no pressure;
(5) cooling for 2 hours to finish the preparation of tungsten copper;
the preparation time in the above steps (1) to (4) was 2 hours.
Example 2
This example differs from example 1 in that:
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 30s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 1020 ℃ at a heating rate of 22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063 deg.C and no pressure.
Example 3
This example differs from example 1 in that:
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 50s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 860 ℃ at a heating rate of 22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063 deg.C and no pressure.
Example 4
This example differs from example 1 in that:
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 10s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 1020 ℃ at a heating rate of 22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1080 deg.c and no pressure.
The tungsten copper (alloy) (Wcu 50%) obtained in the above examples 1-4 was tested by a laser thermal conductivity meter and PPMS, and the test items were thermal conductivity.
And (3) detection results:
the embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Claims (9)
1. A rapid preparation method of high-thermal-conductivity tungsten copper is characterized by comprising the following steps:
(1) filling pure tungsten powder and copper powder filler into the surface of the powder after filling;
(2) regulating the gas pressure to be between 0.3 and 0.6Kg under vacuum or inert gas, and mixing materials;
(3) after the mixing is finished, carrying out deoxidation treatment on the powder;
(4) filling powder into a mould, and sintering:
a pre-pressing section: maintaining the pressure for 10-60s under the condition of pre-pressing of 20 MPa;
a temperature rising section: heating at a speed of 120 ℃/min, changing the heating speed to 55 ℃/min when plasticization begins, increasing the pressure according to 5MPa each time until the pressure is 120MPa, and heating to 600 ℃;
after the plasticizing state is finished, heating to 860 ℃ and 1020 ℃ at the heating rate of 20-22 ℃/min, and maintaining the pressure at 120MPa for 10min per 50-15Kg of powder;
a pressure maintaining section: sintering at 1063-1080 ℃ and under a pressureless state;
(5) cooling for 2 hours to finish the preparation of tungsten copper;
the preparation time of the steps (1) to (4) is 1.5 to 2.5 hours.
2. The method for rapidly preparing tungsten copper with high thermal conductivity according to claim 1, wherein the step (1) is specifically as follows: taking pure tungsten powder and copper powder, placing the copper powder at the bottom, covering the copper powder with the pure tungsten powder to finish filling, and filling a mixing ball on the surface of the powder;
the mixing ball is an alloy ball or a ceramic ball.
3. The method for rapidly preparing high thermal conductivity tungsten copper according to claim 2, wherein when the mixing ball is an alloy ball, the weight ratio of the alloy ball to the powder is 3:1, and the diameter of the alloy ball is phi 10 or phi 18.
4. The rapid preparation method of tungsten copper with high thermal conductivity according to claim 3, characterized in that when the mixture ball is a ceramic ball, the weight ratio of the ceramic ball to the powder is 5:1, the ball diameter of the ceramic ball is phi 3, phi 5 or phi 10; the ceramic balls are zirconium balls.
5. The method for rapidly preparing high thermal conductivity tungsten-copper according to claim 1, wherein the formula ratio of the tungsten-copper is any one of Wcu10, Wcu20, Wcu30, Wcu40 and Wcu 50.
6. The method for rapidly preparing tungsten copper with high thermal conductivity according to claim 1, wherein the step (2) is specifically as follows: when a vacuum method is adopted, the vacuum environment is 10-2And (3) mixing materials for 12 hours by adjusting the air pressure to be between 0.3 and 0.6 Kg.
7. The method for rapidly preparing tungsten copper with high thermal conductivity according to claim 1, wherein the step (2) is specifically as follows: when an inert gas method is adopted, vacuumizing is firstly carried out for 3min, a vacuum valve is closed, an inflation valve is opened, inert gas is inflated, when the pressure is 1K +/-0.1, the inflation valve is closed, inflation is stopped, the air pressure is adjusted to be 0.3-0.6Kg, and the materials are mixed for 12-18 hours.
8. The rapid preparation method of tungsten copper with high thermal conductivity according to claim 1, wherein the requirement of filling the powder in the mold in step (4) is uniform powder filling.
9. The rapid preparation method of tungsten copper with high thermal conductivity according to claim 1, wherein the sintering in step (4) is sintering to keep balance and consistency of upper and lower pressure heads of the die during charging.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045885A (en) * | 2012-12-27 | 2013-04-17 | 中南大学 | Preparation method for high-density fine grain tungsten copper alloy |
| CN104404282A (en) * | 2014-12-02 | 2015-03-11 | 天龙钨钼（天津）有限公司 | Tungsten copper alloy with low tungsten content and preparation method of tungsten copper alloy |
| CN109355541A (en) * | 2018-12-17 | 2019-02-19 | 东北大学 | A method of preparing high density tungsten copper alloy |
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- 2021-06-11 CN CN202110657386.3A patent/CN113881864A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045885A (en) * | 2012-12-27 | 2013-04-17 | 中南大学 | Preparation method for high-density fine grain tungsten copper alloy |
| CN104404282A (en) * | 2014-12-02 | 2015-03-11 | 天龙钨钼（天津）有限公司 | Tungsten copper alloy with low tungsten content and preparation method of tungsten copper alloy |
| CN109355541A (en) * | 2018-12-17 | 2019-02-19 | 东北大学 | A method of preparing high density tungsten copper alloy |
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